Engineering Papers⌕ Search

SEARCH · Engineering Papers

Results for “SAMPLE PREPARATION”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 721 records · Page 40

Properties of the exotic metastable ST12 germanium allotrope

The optical and electronic properties of semiconducting materials are of great importance to a vast range of contemporary technologies. Diamond-cubic germanium is a well-known semiconductor, although other ‘exotic’ forms may possess distinct properties. In particular, there is currently no consensus for the band gap and electronic structure of ST12-Ge (tP12, P4 3 2 1 2) due to experimental limitations in sample preparation and varying theoretical predictions. Here we report clear experimental and theoretical evidence for the intrinsic properties of ST12-Ge, including the first optical measurements on bulk samples. Phase-pure bulk samples of ST12-Ge were synthesized, and the structure and purity were verified using powder X-ray diffraction, transmission electron microscopy, Raman and wavelength/energy dispersive X-ray spectroscopy. Lastly, optical measurements indicate that ST12-Ge is a semiconductor with an indirect band gap of 0.59 eV and a direct optical transition at 0.74 eV, which is in good agreement with electrical transport measurements and our first-principles calculations.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Nanometer Scale Imaging to Develop Quantitative Descriptors of Bipolar Membrane Junction Structure

Swings in pH can be achieved by electrically polarizing a bipolar membrane (BPM) to drive water dissociation at the BPM junction for electrochemical conversion and separation processes. BPM junction design is critical to tailor performance for specific applications; however, characterization techniques capable of resolving the nanometer scale physical structure of the junction are limited. We present sample preparation, imaging, and analysis workflows that are adaptable to a variety of BPM junction architectures. Atomic force microscopy produces BPM junction images with nanometer scale lateral resolution for samples with and without a graphene oxide water dissociation catalyst in the junction. Subsequent image segmentation and analysis quantify line edge roughness and catalyst layer thickness as descriptors of junction structure. Comparison of pre- and post-electrodialysis junctions suggests electric field-induced alignment of catalyst particles during electrodialysis. This characterization workflow can inform manufacturing protocols, computational modeling, and failure mode analysis for next-generation BPMs.

97 MATHEMATICS AND COMPUTING↗

Structural analysis and ferroelectric properties of Fe doped BaTiO{sub 3}

The polycrystalline samples of Fe doped BaTiO{sub 3} (BTO) with compositional formula BaTi{sub 1-x}Fe{sub x}O{sub 3} (x = 0, 0.03, 0.04 and 0.05) were prepared by solid-state reaction route. The influence of the Fe content on the structural, vibrational and electric properties of BaTiO{sub 3} was investigated using X-ray powder diffraction (XRD), Raman spectroscopy and Polarization techniques. XRD analysis indicates the formation of single-phase tetragonal structure for all the prepared samples. Tetragonal cubic structure with space group P4mm of all samples is further approved by Rietveld refinement. Room temperature Raman spectra of pure BaTiO{sub 3} show four active modes of vibration whose intensity decreases with increasing Fe doping. Small shift in Raman modes and increment in the line width has been observed with the doping ions. The hysteresis loop is very well performed with regular sharp characteristic of ferroelectric materials.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Characterization of actinide abundances and isotopic compositions by HR-ICP-MS

In this report, we present actinide isotopic and elemental data from fallout melt glass using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS). This is an analytical technique that requires minimal sample preparation. These data are directly compared to the results of high precision isotopic analyses and elemental assay by multi-collector (MC-) ICP-MS, which requires lengthy sample processing involving spiking and purifying aliquots of individual elements. The comparison shows broad overlap between the results of the two techniques. Thus, although the data obtained by HR-ICP-MS is of significantly lower precision, it is a viable method to obtain actinide elemental and isotopic data on a more rapid timeframe than traditional high-precision techniques.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

COMPAS: Compositional mineralogy with a photoacoustic spectrometer

There is an important need for an in situ method of mineral and rock identification and quantification that provides true absorption spectra for a wide spectral range for lunar lander/rover missions. Many common minerals such as feldspars, magnetite, ilmenite, and amorphous fine solids or glasses, can exhibit flat spectral reflectances in the 400-2500 nm spectral region that render inaccurate or difficult their spectral detection and quantitative analysis. Ideal rock and mineral spectra are, of course, pure absorption spectra that are independent of the spectral effects of scattering, particle size, and distribution that can result in a suppression or distortion of their spectral features. This ideal seldom pertains to real samples. Since sample preparation is difficult and may fundamentally alter the observed diffuse spectral reflectance, an in situ spectral measurement method for rocks and minerals on the Moon, insensitive to the sample morphology, would be invaluable. Photoacoustic spectroscopy is a well-established technique appropriate for this task that has been widely applied in condensed-phase spectral studies of complex, highly light scattering, unprepared samples of everything from coal to whole blood, including rock and mineral characterization. A Compositional Mineralogy Photoacoustic Spectrometer, or COMPAS, can enable in situ spectral measurement of rocks and minerals, bypassing the major limitations of diffuse reflectance spectroscopy. COMPAS spectral capabilities for rock and mineral samples will be incorporated into an instrument prototype specifically for lunar measurements, compatible with rover capabilities.

Smith, W. Hayden↗

Constraints on Exposure Ages of Lunar and Asteroidal Regolith Particles

Mineral grains in lunar and asteroidal regolith samples provide a unique record of their interaction with the space environment. Exposure to the solar wind results in implantation effects that are preserved in the rims of grains (typically the outermost 100 nm), while impact processes result in the accumulation of vapor-deposited elements, impact melts and adhering grains on particle surfaces. These processes are collectively referred to as space weathering. A critical element in the study of these processes is to determine the rate at which these effects accumulate in the grains during their space exposure. For small particulate samples, one can use the density of solar flare particle tracks to infer the length of time the particle was at the regolith surface (i.e., its exposure age). We have developed a new technique that enables more accurate determination of solar flare particle track densities in mineral grains <50 micron in size that utilizes focused ion beam (FIB) sample preparation combined with transmission electron microscopy (TEM) imaging. We have applied this technique to lunar soil grains from the Apollo 16 site (soil 64501) and most recently to samples from asteroid 25143 Itokawa returned by the Hayabusa mission. Our preliminary results show that the Hayabusa grains have shorter exposure ages compared to typical lunar soil grains. We will use these techniques to re-examine the track density-exposure age calibration from lunar samples reported by Blanford et al. (1975).

Berger, Eve L.↗

Copper(II) imidazolate frameworks as highly efficient photocatalysts for reduction of CO{sub 2} into methanol under visible light irradiation

Three copper(II) imidazolate frameworks were synthesized by a hydrothermal (or precipitation) reaction. The catalysts were characterized by X-ray diffraction (XRD), nitrogen adsorption, transmission electron microscopy (TEM), ultraviolet–visible spectroscopy (UV–vis), Fourier transform infrared spectra (FTIR), thermogravimetry (TG). Meanwhile, the photocatalytic activities of the samples for reduction of CO{sub 2} into methanol and degradation of methylene blue (MB) under visible light irradiation were also investigated. The results show that the as-prepared samples exhibit better photocatalytic activities for the reduction of carbon dioxide into methanol with water and degradation of MB under visible light irradiation. The orthorhombic copper(II) imidazolate frameworks with a band gap of 2.49 eV and green (G) color has the best photocatalytic activity for reduction of CO{sub 2} into methanol, 1712.7 μmol/g over 5 h, which is about three times as large as that of monoclinic copper(II) imidazolate frameworks with a band gap 2.70 eV and blue (J) color. The degradation kinetics of MB over three photocatalysts fitted well to the apparent first-order rate equation and the apparent rate constants for the degradation of MB over G, J and P (with pink color) are 0.0038, 0.0013 and 0.0016 min{sup −1}, respectively. The synergistic effects of smallest band gap and orthorhombic crystal phase structure are the critical factors for the better photocatalytic activities of G. Moreover, three frameworks can also be stable up to 250 °C. The investigation of Cu-based zeolitic imidazolate frameworks maybe provide a design strategy for a new class of photocatalysts applied in degradation of contaminations, reduction of CO{sub 2}, and even water splitting into hydrogen and oxygen under visible light. - Graphical abstract: Carbon dioxide was reduced into methanol with water over copper(II) imidazolate frameworks under visible light irradiation. - Highlights: • Three copper(II) imidazolate frameworks were first applied in the photo-reduction of CO{sub 2}. • The photocatalytic activities of the frameworks depend on their band gap and phase structures. • The photocatalytic activity of orthorhombic frameworks is 3 times that of monoclinic frameworks. • The degradation kinetics of MB over three photocatalysts followed the first-order rate equation. • The largest yield for reduction of CO{sub 2} into methanol on green framworks was 1712.7 μmol/g over 5 h.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Zn interstitial defects induced magnetic nature in Fe ions doped ZnO based DMS

This paper describes the synthesis of Fe doped ZnO samples Zn{sub 1-x}Fe{sub x}0, where x various from 0.01≤x≤0.05 (in steps of 0.01) by solution method. The effect of Fe ions doping on the structural, optical and magnetic properties was investigated using X-ray diffraction (XRD), Photoluminescence and vibrating sample magnetometer (VSM) measurements. The observed result indicates that the samples are single phase formation of the wurtzite structure without any significant secondary phase in it. The photoluminescence spectra reveals the presence of Zn vacancies. The magnetic property of prepared samples was studied using a vibrating sample magnetometer and the observed results revealed a super-paramagnetic behavior for the Fe doped ZnO samples.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Nanometer-Scale Imaging of Inhomogeneous Active Charge Carriers in Arsenic-Doped CdTe Thin Films

We report nanometer-scale imaging of active carrier distribution of As-doped CdTe films by scanning capacitance microscopy (SCM). We developed SCM sample preparation for CdTe by ion-milling followed by thermal processing. The nanometer-resolution carrier delineation for CdTe was validated by imaging on a CdTe cross-section sample made by a molecular beam epitaxy layer stack with As-doping concentrations of 10^15 ~10^18 /cm 3 . We found that the carrier distribution in As-doped films was significantly nonuniform, with inhomogeneity ranging from sub-um to a few um and concentration variation of one order of magnitude (low 10^16 to low 10^17 /cm 3 ). This nonuniformity is distributed randomly, independent of grain structure and grain boundary (GB). We used Kelvin probe force microscopy (KPFM) and cathodoluminescence (CL) to further map the surface potential and radiative illumination on the same area as the SCM image. Higher potential and lower CL intensity were found on GBs but not on SCM contrast, illustrating positive GB charging and GB recombination but not GB-distinguished doping. The overall KPFM potential image is in rough agreement with the SCM carrier distribution, in terms of Fermi-level position relative to the bandgap edge - thus resulting in the band-edge potential fluctuation. Nonuniform carrier concentration, potential fluctuation, and defect recombination can all together cause the Voc deficit of the As-doped CdTe device.

14 SOLAR ENERGY↗

Magic Angle Spinning NMR Metabolomics

Nuclear Magnetic Resonance (NMR) spectroscopy is a non-destructive, quantitative, reproducible, untargeted and unbiased method that requires no or minimal sample preparation, and is one of the leading analytical tools for metabonomics research [1-3]. The easy quantification and the no need of prior knowledge about compounds present in a sample associated with NMR are advantageous over other techniques [1,4]. 1H NMR is especially attractive because protons are present in virtually all metabolites and its NMR sensitivity is high, enabling the simultaneous identification and monitoring of a wide range of low molecular weight metabolites.

Environmental Molecular Sciences Laboratory↗

Structural differences existing in bulk and nanoparticles of Y{sub 2}Sn{sub 2}O{sub 7}: Investigated by experimental and theoretical methods

Present manuscript deals with the structural changes associated with transformation of bulk Y{sub 2}Sn{sub 2}O{sub 7} into nanoparticles of Y{sub 2}Sn{sub 2}O{sub 7}. Nanoparticles of Y{sub 2}Sn{sub 2}O{sub 7} both undoped and Eu{sup 3+} doped, were prepared at a relatively low temperature (700 °C) and investigated for their structural and luminescence properties and compared them with that of bulk Y{sub 2}Sn{sub 2}O{sub 7} sample prepared by the solid-state method at 1300 °C. Significant distortion in geometry and electron density distribution around Y{sup 3+}/Eu{sup 3+} ions in nanoparticles are confirmed from the Rietveld refinement of the powder X-ray diffraction patterns and theoretical calculations based on the density functional theory (DFT). The SnO{sub 6} octahedron in Y{sub 2}Sn{sub 2}O{sub 7} is more expanded in nanoparticles compared to bulk. Iso-surface density distribution reveals that while bulk sample shows typical ionic feature in Y/Eu--O bonds, nanoparticle sample shows sharing of electron density along bond axis pertaining to covalent character. These inferences are further supported by the doped Eu{sup 3+} luminescence and calculated Ω{sub 2} and Ω{sub 4} parameters. - Graphical abstract: YO{sub 8} scalenohedron present in bulk and nanoparticles of Y{sub 2}Sn{sub 2}O{sub 7}.Variation of the electron density around Y{sup 3+} ions in YO{sub 8} polyhedron is also shown in bulk and nanoparticles of Y{sub 2}Sn{sub 2}O{sub 7}. The difference in the extent of ionic/covalent nature of the Y--O bond is clearly seen the contour plot of electron density. Highlights: ► YO{sub 8} scalenohedron is axially and equatorially distorted in Y{sub 2}Sn{sub 2}O{sub 7} nanoparticles. ► Enlargement of SnO{sub 6} octahedron in nanoparticles of Y{sub 2}Sn{sub 2}O{sub 7} compared to bulk. ► Less symmetric charge distribution around Y{sup 3+} ions in Y{sub 2}Sn{sub 2}O{sub 7} nanoparticles.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

The Preparation of Non-radioactive Glassy Surrogate Nuclear Explosion Debris (SNED) Loaded with an Isotopically Altered Noble Gas

The measurement of the Kr and Xe isotope ratios in nuclear explosion debris is an important forensic tool as the method requires very little sample preparation. Fragments of debris are simply crushed or heated to release the trapped gases Kr and Xe arising from fission product decay. As suitable test materials are not readily available we have been investigating a method to incorporate isotopically enriched 129Xe in glassy materials that mimic nuclear explosion debris. The approach used to prepare these materials will be described along with some of the example results obtained.

Trinitite, Nuclear forensics, Fission Xe, Surrogat↗

Investigation of Electrical and Magnetic Properties of La{sup 3+} Substituted M-Type Ba–Ni Nano-Ferrites

In this paper, La{sup 3+} substituted M-type Ba–Ni hexaferrite nanoparticles having composition Ba{sub 0.8}Ni{sub 0.2}Fe{sub 12-x}La{sub x}O{sub 19} (x = 0, 0.2, 0.4, 0.6, and 0.8) were prepared by co-precipitation route. The phase of the grown NPs was confirmed using X-ray diffraction analysis and results reveal the growth of M-type hexaferrite NPs as a major phase. The energy dispersive X-ray spectroscopy (EDX) was employed to determine the elemental composition of prepared samples. The FTIR spectra of synthesized samples confirm the bond formation of M-type hexaferrites. The optical bandgap was determined by UV-Vis spectroscopy and the results exhibit an increase in optical bandgap with decreasing crystallite size. The vibrating sample magnetometry (VSM) technique was used to analyze the effect of dopant on the magnetic properties like coercivity, saturation magnetization, and remanence of the synthesized samples. The electrical resistivity was measured by two probe method and it was observed that the activation energy shows a decreasing trend with increase in La content. The highly resistive nature of prepared nano ferrites indicates the potential to use these ferrites for high-frequency applications.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Molecular weight dependent structure and charge transport in MAPLE-deposited poly(3-hexylthiophene) thin films

In this work, poly(3-hexylthiophene) (P3HT) films prepared using the matrix-assisted pulsed laser evaporation (MAPLE) technique are shown to possess morphological structures that are dependent on molecular weight (MW). Specifically, the structures of low MW samples of MAPLE-deposited film are composed of crystallites/aggregates embedded within highly disordered environments, whereas those of high MW samples are composed of aggregated domains connected by long polymer chains. Additionally, the crystallite size along the side-chain (100) direction decreases, whereas the conjugation length increases with increasing molecular weight. This is qualitatively similar to the structure of spin-cast films, though the MAPLE-deposited films are more disordered. In-plane carrier mobilities in the MAPLE-deposited samples increase with MW, consistent with the notion that longer chains bridge adjacent aggregated domains thereby facilitating more effective charge transport. The carrier mobilities in the MAPLE-deposited simples are consistently lower than those in the solvent-cast samples for all molecular weights, consistent with the shorter conjugation length in samples prepared by this deposition technique.

36 MATERIALS SCIENCE↗

Structural, photoluminescence and radioluminescence properties of Eu{sup 3+} doped La{sub 2}Hf{sub 2}O{sub 7} nanoparticles

This study presents the structural, optical, and radioluminescent characterization of newly synthesized europium-doped lanthanum hafnate (La{sub 2}Hf{sub 2}O{sub 7}:xmol%Eu{sup 3+}, x=0 to 35) nanoparticles (NPs) for use as phosphors and scintillation materials. Samples prepared through a combined co-precipitation and molten salt synthetic process were found to crystalize in the pyrochlore phase, a radiation tolerant structure related to the fluorite structure. These samples exhibit red luminescence under ultraviolet and X-ray excitation. Under these excitations, the optical intensity and quantum yield of the La{sub 2}Hf{sub 2}O{sub 7}:xmol%Eu{sup 3+} NPs depend on the Eu{sup 3+} concentration and are maximized at 5%. It is proposed that there is a trade-off between the quenching due to defect states/cross-relaxation and dopant concentration. An optimal dopant concentration allows the La{sub 2}Hf{sub 2}O{sub 7}:5 mol%Eu{sup 3+} NPs to show the best luminescent properties of all the samples. - Graphical abstract: Incident X-ray and UV photons interact with La{sub 2}Hf{sub 2}O{sub 7}: xmol%Eu{sup 3+}(x=1–35) nanoparticles (NPs) to yield strong red luminescence centered at 612 nm. Colored spheres inside NP diagram represent pyrochlore coordination environment of La{sub 2}Hf{sub 2}O{sub 7}:xmol%Eu{sup 3+}. Blue, red, yellow, green and black spheres represent hafnium(IV) atoms, lanthanum(III)/europium(III) atoms, oxygen atoms at 48f site, oxygen atoms at 8b site and oxygen vacancies, respectively. - Highlights: • La{sub 2}Hf{sub 2}O{sub 7}:xmol%Eu{sup 3+} (x=0–35) nanoparticles with weakly-ordered pyrochlore structures were synthesized. • Optically and X-ray excited emission spectra showed strong luminescence centered at 612 nm. • Photoluminescence quantum yield increases with doping concentration up to 5% and decreases at higher concentrations.

36 MATERIALS SCIENCE↗

Ultra-high SERS detection of consumable coloring agents using plasmonic gold nanostars with high aspect-ratio spikes

Solution-based SERS detection by using a portable Raman instrument has emerged as an important tool due to its simplicity, and flexibility for rapid and on-site screening of analyte molecules. However, this method has several shortcomings, including poor sensitivity especially for weak-affinity analyte molecules, where there is no close contact between the plasmonic metal surface and analyte molecule. Examples of weak-affinity molecules include pigment molecules that are commonly used as a consumable coloring agent, such as allura red (AR), and sunset yellow (SY). As high consumption of colorant agents has been shown to cause adverse effects on human health, there is a strong need to develop a simple and practical sensing system with high sensitivity for these agents. Here we present a novel, highly sensitive solution-based SERS detection method for AR, and SY by using CTAC capped gold nanostars (GNS) having different aspect ratios (GNS-2, GNS-4, and GNS-5) without utilizing any aggregating agents which can enhance SERS signal however it reduces batch to batch reproducibility. The influence of the aspect ratio of GNS on SERS properties was investigated. We have achieved a limit of detection (LOD) of AR and SY as low as 0.5 and 1 ppb, respectively by using GNS-5 with the advantages of minimal sample preparation by just mixing the analyte solution into a well plate containing GNS solution. In addition, excellent colloidal stability and reproducibility have further enhanced the applicability in real-world samples. Altogether, our results evidence that the solution-based SERS detection platform using high aspect-ratio GNS can be applied for practical application to detect pigment molecules in real samples with satisfactory results.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

The changes in optical absorbance of ZrO{sub 2} thin film with the rise of the absorbed dose

In this study, zirconium oxide (ZrO{sub 2}) thin film samples prepared by sol–gel method were irradiated using Co-60 radioisotope as gamma source. Then, it was investigated the ionizing effect on optical properties of ZrO{sub 2} thin film samples with the rise of the absorbed dose. The changes in the optical absorbance of ZrO{sub 2} thin films were determined by using optical transmittance and the reflectance measurements in the range between 190 – 1100 nm obtained from PG Instruments T80 UV-Vis spectrophotometer.

36 MATERIALS SCIENCE↗

Inhomogeneous Magnetic State of Ce{sub 2}Fe{sub 17} Evidenced by Mössbauer Spectroscopy

A comparative analysis of the magnetic properties and Mössbauer spectra of two Ce{sub 2}Fe{sub 17} samples prepared by different methods and demonstrating different magnetic behavior is carried out. A model for processing the spectra is proposed, which gives a good description of the Mössbauer spectra of samples in different magnetic states by a superposition of eight subspectra. It is shown that in the samples in the ferromagnetic state there are regions with antiferromagnetic ordering at the local level. The relative fractions of iron atoms in these regions differs for different samples and increases when approaching the temperature of the transition from the ferromagnetic to the antiferromagnetic state.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗